Process of hydrolysis, particularly the splitting of oils and fats



Patented Jan. 24, 1928.

UNITED STATES PATENT OFFICE.

- PEBCIVAL JOHN FRYE'R, F K'EN'I, ENGLAND, ABSIGNOR '10 CATALPO LIKI'I'ID, OI LONDON, ENGLAND, A BRITISH LIMITED LIABILITY COMPANY.

PBOGESS 0]! HYDROLYSIS, PARTICULARLY THE SPLITTING OI OILS AND FATS;

No Drawing. Application filed April 9, 1921, Serial No. 460,089,-and in Great Britain April 24, 1990.

According to this invention, a process of hydrolysis or saponification, for example,-

the hydrolysis of an oil or fat,-is characterized by efiecting the reaction in the presence of clay in a state of fine subdivision.

Advantageously, a clay of high purity is employed. Such clay. which for convenience will be hereafter referred to as colloidal clay, may be obtained from any suitable natural clay by washing and sedimentation, or other process which is adapted to yield a pure product and enhance the colloidal nature of the original substance, and, preferably, the clay used is one which has been prepared by aid of peptiz'ation. For example, a clay which has been submitted to the treatment described in Feldenheimers British specification No. 106,890, or United States Patent No. 1,324,958 of December 16,

1919, may with advantage be utilized.

By peptization is meant the dispersion of the clay in a fluid medium by addition of an appropriate quantity of a deflocculating reagent, for example, ammonia, sodium hy- .drate, orsodium carbonate. The clay substance isthen recovered from its suspension in any known way.

The hydrolysis may be carried out under any appropriate conditions of temperature 6 and pressure, and byaid of the usual hydrolyzing accelerating agents, such as bases, alkalis (for example, lime, sodium and potassiumhydroxide, sulpho-aromatic or sulpho-fatty compounds (for example, Twitchells reagent) litholytic ferments (of whlch the ferment of castor-oil seeds is a notable example), or other reagents as may be desired.

The proportion of clay utilized may be varied according to circumstances as, for 1nstance, the nature of the substance under treatment and the particular composition of the reaction mixture.

One form of clay suitable for carrying the present invention into effect 1s, as already stated obtained by the process described in British specification No. 106,890 or United States Patent No. 1,324,958. For instance,

the following procedure may be followed.

A high-class china clay, such as Fraddon 5 clay, is washed by passing it over micasure for upwards of drags in the usual manner,-but instead of water only, a solution of 1.2 parts by weight ofsodium carbonate (calculated as anhydrous salt) in 2000 parts by weight of water is utilized for 100 parts, or 5 per cent clay suspenslon. A lar er quantity of mica? is deposited upon t e drags than is so removedwhen water alone is employed. The clay dispersion passes to a settling-tank'in whlch it is left to stand for further deposition of mica, and thence is led to a second tank where the clay is precipitated by appropriate addition of a precipitant, for example, a weaksolution of alum.

The peptizing agent, i. e. the sodium car- 7 'bonate, may obviously also be added at any other vdesired stage before leading the suspension over the drugs Alternatively, the peptizing agent may be added prior to entry of, the suspension into the settling-tank after the customary treatment on the mica-drags, the liquid being allowed to stand in this tank for a sufiicient penod of time, and the clay dispersion being then run into the tank where the flocculating reagent is added.

In place of sodium carbonate, other peptizing agents may be employed, such, for example, as ammonia.

There results from this treatment a very highly purified and finely divided clay, and the following are examples of the use of this particular clay for carrying the present in vention into efiect, it being understoodthat these examples are given for illustrative purposes and not by way of limitation.

Ewample I 45 lbs. of the colloidal clay and 450 lbs. of zinc oxide are worked up into a thin paste with about 15 cwt. of water inan agitator, and the paste is transferred to an autoclave containing 3 tons of cottonseed oil. Steam under pressure, which need not exceed lbs. per' sq. inch, is then introduced and the materials are heated together under presabout 8 hours. per cent of'the oil is thereby resolved into glycerine and fatty acids, together with a certain proportionof zinc soap corresponding to the quantity of zinc oxide used.

It appeared-that the addition of the colloidal clay expedited the process as-well as 1 effecting a high degree of hydrolysis with a consequent superior yield of glycerine, while 110 ture.

Ewample I I Known weights of the following oils were heated at about 100 C. for the following periods with a given volume of a standard solution of caustic soda in excess. The same oils were similarly treated for the same period of time and under identical conditions in presence of the colloidal clay. The degree of saponification in each case was then determined by titration of the excess of alkali. The following results were ob tamed Per cent oil Tlme (hrs. Per cent clay i mine). (on oil). E23

01M Oil. L 15 0. O i 22. 6 1. l5 9. 0 53. 2 1. 15 O. O i1. 0 1. 15 1s. 0 52. o

Limud oil. 1. O O. 0 39. 6 1. O I. 0 97. 3

Cotton seed oil. 1. 0 0. 0 6. 7 1. 0 11. O 58. 8 1. 30 0. 0 9. 9 1. m 11. O 87. 0 1 U 0. 0 12. 3 2. 0 11. 0 97. 4

When desired, at the conclusion of the process, the clay may be removed by settlement or filtration or in any other suitable way, but in the case of saponification of an oil or fat by means of alkalis it will freuently be found advantageous to retain the c ay in the finished soap since the" properties of the latter are thereby improved.

What I claim as my invention and desire to secure by Letters Patent is:-

1. A process of hydro] sis of liquid lycerides of fatty acids w erein the hydrolytic reaction is effected b heating under ressure in the presence 0 clay which has een prepared by aid of peptization.

2. A process of hydrolysis of liquid glycerides of fatty acids wherein the hydrolytic reaction is efl'ected by heating under pressure in the presence of clay which has been prepared by aid of peptization with an alraline clay-peptizing agent.

3. A process of hydrolysis of liquid glycerides of fatty acids wherein the hydrolytic reaction is efiected by heating under pressure with a hydrolysis accelerator in the presence of clay which has been prepared by aid of peptization.

4. A process of hydrolysis of liquid glycerides of fatty acids wherein the hydrolytic reaction is effected by heating under pres sure with a hydrolysis accelerator in the presence of clay which has been prepared by aid of peptization with an alkaline claypeptizing agent.

5. A process of hydrolysis of liquid glycerides of fatty acids wherein the hydrolytic reaction is effected by heating under pressure with an alkaline hydrolysis accelerator in the presence of clay which has been prepared by aid of peptization.

6. A process of hydrolysis of liquid glycerides of fatty acids wherein the hydrolytic reaction is effected by heating under pressure with an alkaline hydrolysis accelerator in the presence of clay which has been prepared by aid of peptization with an alkaline clay-peptizing agent.

In testimony whereof I afiix my signature.

PEROIVAL JOHN FRYER. 

